Sains Malaysiana 55(8)(2026): 1363-1371

http://doi.org/10.17576/jsm-2026-5508-11
 

Analisis Residu 2-Fenilfenol dan 4-Fenilfenol dalam Buah Sitrus Menggunakan Kaedah Pengekstrakan Mikro Cecair-Cecair Tersebar (DLLME) dan Spektrofotometri Ultraungu-Boleh Nampak (UV-VIS)

(Analysis of 2-Phenylphenol and 4-Phenylphenol Residues in Citrus Fruits Using Dispersed Liquid-Liquid Micro-Extraction (DLLME) and Ultraviolet-Visible Spectrophotometry (UV-VIS)

 

NUR ALIFFAH ANISSA BINTI MOHD FAUZI, NADHIRATUL-FARIHIN BINTI SEMAIL* & FAIQ HAFIY BIN ROZEMAN

 

Jabatan Sains Kimia, Fakulti Sains dan Teknologi, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

 

Diserahkan: 18 Mei 2026/Diterima: 16 Ogos 2026

 

Abstrak

Antioksidan fenol merupakan antara unsur yang banyak terdapat dalam buah-buahan yang memberikan pelbagai manfaat kesihatan kepada pengguna. Bagi menentukan kandungan dan taburan 2- dan 4-fenilfenol dalam lima jenis jus buah sitrus, satu kaedah yang pantas, sensitif serta mesra alam iaitu pengekstrakan mikro cecair-cecair secara serakan (DLLME) telah digunakan di bawah keadaan optimum pH 5, 1.5 g NaCl, 1.5 mL isopropanol sebagai pelarut penyebar dan 1.2 mL diklorometana sebagai pelarut pengekstrak. Analisis preliminari menggunakan kromatografi lapisan nipis (TLC) dengan menggunakan toluena dan aseton (8:2) sebagai pelarut fasa bergerak telah dijalankan bagi penvisualisasi 2 dan 4-fenilfenol di bawah cahaya ultraungu. Namun begitu, disebabkan kedua-dua analit mempunyai kepekatan yang sangat rendah, ia tidak dapat dikesan melalui kaedah TLC. Ujian DPPH tidak menunjukkan perubahan warna yang signifikan, yang menunjukkan bahawa kepekatan antioksidan dalam sampel sitrus mungkin terlalu rendah untuk dinilai secara berkesan menggunakan kaedah ini tanpa proses prapekatan sampel. Oleh itu, kaedah kuantifikasi menggunakan DLLME dan spektrofotometer UV-Vis pada panjang gelombang 245 dan 287 nm telah dijalankan. Jus lemon menunjukkan kepekatan 2- dan 4-fenilfenol  yang tertinggi antara kelima-lima sampel buah dengan nilai 0.0212 dan 0.0371 mg/mL masing-masing bagi 2 dan 4-fenilfenol. Keputusan menunjukkan kedua-dua analit mempunyai pekali kolerasi linear (R²) 0.9917 dan 0.9899. Had pengesanan (LOD) dan had pengkuantifikasian (LOQ) masing-masing adalah 0.00119 dan 0.00408 bagi 2-fenilfenol manakala 0.00127 dan 0.00436 bagi 4-fenilfenol. Peratusan penghasilan semula adalah dari 85.92 sehingga 105.5% bagi 2-fenilfenol dan 90.30 sehingga 114.8% bagi 4-fenilfenol dengan sisihan piawai relatif harian (RSD) 0.1977 hingga 0.5189. Kaedah ini telah berjaya digunakan untuk analisis sampel sebenar jus buah dan membuktikan bahawa teknik ini adalah teknik yang ringkas, pantas dan praktikal serta mesra alam.

Kata kunci: Antioksidan fenol; buah sitrus; DLLME; UV-Vis; TLC

 

Abstract

Phenolic antioxidants are among the many compounds found in fruits that offer various health benefits to consumers. To determine the content and distribution of 2- and 4- phenylphenol in five types of citrus fruit juices, a rapid, sensitive, and environmentally friendly method, dispersive liquid-liquid microextraction (DLLME) was employed under optimized conditions: pH 5, 1.5 g of NaCl, 1.5 mL of isopropanol as the disperser solvent, and 1.2 mL of dichloromethane as the extractant solvent. A preliminary analysis was conducted using thin-layer chromatography (TLC) with toluene and acetone (8:2) as the mobile phase solvent to visualize 2- and 4-phenylphenol under ultraviolet light. However, due to the very low concentrations of both analytes, they could not be detected by TLC. The DPPH assay also did not exhibit a significant colour change, suggesting that the antioxidant compounds in the citrus sample may be present at concentrations too low for effective detection using this method without prior sample pre-concentration. Therefore, quantification was carried out using UV-Vis spectrophotometry at wavelengths of 245 and 287 nm. Lemon juice showed the highest concentrations among the five fruit juice samples, with values of 0.0212 and 0.0371 mg/mL for 2- and 4-phenylphenol, respectively. The results showed that both analytes had linear correlation coefficients (R²) of 0.9917 and 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.00119 and 0.00408 for 2-phenylphenol, and 0.00127 and 0.00436 for 4-phenylphenol, respectively. The recovery percentages ranged from 85.9 to 105.5% for 2-phenylphenol and 90.3 to 114.8% for 4-phenylphenol, with daily relative standard deviations (RSD) ranging from 0.1977 to 0.5189. This method was successfully applied to the analysis of real fruit juice samples and demonstrated that it is a simple, rapid, practical, and environmentally friendly technique.

Keywords: Citrus fruit; DLLME; phenolic antioxidant; TLC; UV-Vis

 

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*Pengarang untuk surat-menyurat; email: nadhiratulfarihin@ukm.edu.my

 

 

 

 

 

 

 

           

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